Method for producing basic titanic-sulfate products and pure titanic oxid therefrom.



UNITED STATES PATENT OFFICE. tours n. nanroN, or NIAGARA rants, Nnw roux, As'sIcNoa ro THE TITANIUM ALLOY MANUFACTURING COMPANY, on NEW roux, Y., A -CORPOBATION or MAINE.

METHOD FOR PRODUCING BASIC TITANIC-SULFATE PRODUCTS ANDPUBE TITANIC i THEBEFBOM.

v Specification of Letters latent 1 Patented Ap 1917.

Ho Drawing. Application filed August 29, 1916. Serial 170. 117,399.

To all whom it may concern.-

Be it knownthat I, LOUIS E. BARTON, a citizen of the United States, and'a resident of Niagara Falls, in the county of Niagara andStat'e of New York, have invented a certain new and useful Method for Producing Basic Titanic-Sulfate Products and Pure-Titanic Oxid Therefrom, of which thefollowing is a specification. l U

My present invention relates to methods for producing,in industrially important and useful quantities, substantially pure titanic oxid, and by production,la'nd,utilization, to

that end of substantially such an essentially.

basic titanic sulfate product as is described and claimed in the herewith copending application ,of Auguste J. Rossi and myself,

Serial Number 77,469, filed February 10, 1916, the same being a division of our original ap lication Serial Number 7 33,943, filed Novem r 29,1912; and the'objects of my present invention comprise provision of I methods whereby such products are obtainablemore rapidly, certainly, economically, and of better properties, including higher titanic percentages, than heretofore.

In the herewith copendin application of said Rossi and myself, Seria Number 13,47 8,

filed March .10, 1915, is described, and claimed, a method of producing such basic titanic sulfate products by aid of proper dilution and boiling of a titanic sulfate solu-v tion, whereby there is therein precipitated a basictitanic sulfate, and in our sa d application Serial No. 733,943, we have also described, and claimed, another method for a similar purposeby aid of properly' diluting a titanous sulfate, solution and boilingit. in

' presence of'an oxidiz-in agent such as the atmosphere, or, preferab y, nitric acid.

My present method, is distinguishable from these, and from all others known to me, by reason of..its utilizing my discoveries that titanic sulfate solutions' can 'be usefully, if

not always entirely, reduced totitanous sulfate 'solutionsby electrolysis, and-this byaidof merely passing therethrough an electric current between a pair of therewith-contacting electrodes, as distinguished from emg a diaphragm, or .diap'hragm'cell;

P an that, while such solution isbcmg thus addingpractised as follows: I v

I first produce a tltanic sulfate solution,

.electrolyzed, mere heatin' thereof, distinguished from boiling, is sufficient to insure therein precipitation of as much basic titanlc sulfate .as required, and the thereafter 'obtainment, from such precipitate, of a final dried basic titanic product at less expense than heretofore and of superior qual- 1ty and properties, including particularly greater purity than any known to me.

It is also to be noted that my present method adyantageously enables solutions more concentrated. than heretofore to be employed, and results in correspondingly larger yield of the desired final product from a given operation; also that my dispensing with boilingtemperatures is correspond.- ingly economical.

able to, suitably electrolyze without resort to a diaphragm willalso be understood, and

' particularly as regards economy in construetion ,and maintena-nce,'as well asin power.- Nor, by my present method, is there need of sulfuric acid to the solutionj'as in some instances theretofore.

Furthermore, my present method provides relatively ideal c ondi-f titanous sulfate. The advantages of being The process of my: present invention is 5' in any convenient manner, and from any titaniferous material; but I prefer to do this by dissolving in sulfuric acidthe titanic acid product of the method described and claimed in Letters Patent No. 1,171,542, granted to said Rossi-and myself'on February-15, I916; because the titanic sulfate solution thus. ob-

tained isparticularlyfree from impurities, and contains little, if any, free sulfuric acid, .and about 11% of titanic oxid.

is or whatever other solution I employ, I- dilute for various reasons, including the thereby expediting'of the subsequent operations, to

until it contains say about 3% of titanic] .oxid. I have, however, found it preferable,

purpose of subsequently precipitating basic titanic sulfate, an addition of lime chemically equivalent to of the total sulfate in solution is sufficient. After the addition thereto of what may be termed lime-cream, I allow the charge to stand for, 'say, from about one-quarter to one-half of an hour, during which I agitate it from time to time, if only for the purpose of insuring a more complete combination. of the ingredients.

, that a current of from 5 to 10 volts, and 0f.

steam. But I can obtain,

The resulting calcium sulfate I then filter out, and dilute the filtrate so that it shall contain, as in the previously referred to instance, about 3% of titanic oxid.

The sulfate solutions, thus including either of mine above described, I then electrolyze. This, as aforesaid, I refer to accomplish by aid of passing theret rough an electric current between a pair of electrodes immersed in, or contacted the solution. In so doing I, usually, employ a pair of metallic, preferably lead, electrodes, in an undiaphragmed electric cell, and While the voltage may be varied quite considerably, I have discovered a current density at the amperes per square foot, gives satisfactory results. It will be noted that I thus utilize my discovery that in the required treatment, for my purposes, of the solutions employed, a diaphragm, or a diaphragmed cell, is dis pensable.

During the aforesaid electrolysis, I heat, as distinguished from boiling, my solution. Such heating, preferably up to from say 90 C. to 95 manner, .as, for example, by in ecting live in some instances, and according to conditions, passable results with temperatures a little lower than those mentioned. Higher temperatures may be used even up to boiling, though such higher temperatures are, for reasons above referred to and others, rarely, if ever, de-

anode of about 30 p sirable.

. time required will, of

In my operations of my said process, I have obtained yields of from 85% to 90% of the total titanic oxidin the solution in from two and a half to five hours; but the the current conditions.

My resulting precipitate of basic titanic This final product ofmy. present process sulfate solution, 7

., I eflect in any convenient course, in each specific. instance, depend upon the temperatureand is devoid of iron and other impurities, except negligibly, and, as stated in Serial No. 77,469, above referred to, usually contains, by analysis Titanic oxid to Sulfuric anhydrid 5% to 10% Combined water 15% to20% This product I, for certain purposes, calcine, to substantially complete dehydration, at say about 750 0., thereby obtaining a further product which consists essentially of pure titanic oxid (TiO The relative success of my present process, as compared with all others known to me, is, I believe, largely attributable to the alternate reduction and re-oxidation of the.

' neously heated.

am aware that Letters Patent No. 758,710, granted to Howard Spence, May 3rd, 1904:, purport to disclose the reduction of titanic sulfate solutions to titanous sulfate solutions by aid of using the former as a catholyte, and thereby electrolyzing it in a diaphragm cell, and this step I do not wish to be understood as constituting, by itself, any part of my invention, or as covcred by my herein claims.

What I claim as new and desire to secure by Letters Patent is the following, viz:

1. The method of obtaining basic titanic sulfate which comprises electrolyzing a titanic sulfate solution, and meanwhile heating it. i 2. The method of obtaining basic titanic sulfate which comprises electrolyzing a titanicsulfatesolution, and meanwhile heating it to temperatures below boiling.

3. The method of obtaining basic titanic sulfate which comprises adding slaked lime.

to a, titanic sulfate solution, filtering out resulting calcium sulfate, electrolyzing the resulting filtrate, and heating it to temperatures below boiling.

.5. The method of treating a titanic sulfate solution which comprises passing an electrical current therethrough between a meanwhile heating it.

pairof thereby-contacted electrodes, and electrolyzing and heating a titanic solution, meanwhile heating the solution. and thereafter separating therefrom, and

6. The inethod of treating a titanic solucalcining, the resulting precipitate." tion which comprises electrolyzing it, and 4 LOUIS E. BARTON.

, Witnesses: 4 7. The method of producing a titanic oxid Tom C."GRAHAM,

product which comprises simultaneously GEORGE A. OSTERTAG. 

